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WO1996011288A1 - Systeme de revetement par couches nanometriques multiples - Google Patents

Systeme de revetement par couches nanometriques multiples Download PDF

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Publication number
WO1996011288A1
WO1996011288A1 PCT/US1995/012771 US9512771W WO9611288A1 WO 1996011288 A1 WO1996011288 A1 WO 1996011288A1 US 9512771 W US9512771 W US 9512771W WO 9611288 A1 WO9611288 A1 WO 9611288A1
Authority
WO
WIPO (PCT)
Prior art keywords
coating
layers
alumina
component
coatings
Prior art date
Application number
PCT/US1995/012771
Other languages
English (en)
Inventor
Richard S. Mullin
William P. Allen
Maurice L. Gell
Richard H. Barkalow
Allan A. Noetzel
John W. Appleby
Abdus S. Khan
Original Assignee
United Technologies Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by United Technologies Corporation filed Critical United Technologies Corporation
Publication of WO1996011288A1 publication Critical patent/WO1996011288A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/568—Transferring the substrates through a series of coating stations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
    • F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
    • F01D5/12—Blades
    • F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
    • F01D5/288—Protective coatings for blades
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick

Definitions

  • the invention relates to the field of thermally protective coatings and especially to such coatings for use at extreme temperatures.
  • thermal barrier coatings is applied by plasma spraying.
  • a coating there is typically a thin layer, called a bond coat, of a metallic material applied to the substrate, followed by a plasma spray coating of a ceramic material.
  • the metallic bond coat may be applied by various methods including EBPVD (electron beam physical vapor deposition) and plasma spraying.
  • the metallic bond coat composition is selected to maximize the adherence of the plasma sprayed ceramic coating and maximize environmental protection of the substrate in the event of ceramic spallation.
  • Such coatings are typified by U.S. Patent RE 32, 121.
  • thermal barrier coating consists of a ceramic coating applied by EBPVD (electron beam physical vapor deposition). It is a characteristic of the EBPVD process that fissures or cracks appear in the coating during deposition and these fissures divide the 'coating into what amounts into a large number of individual ceramic columns. Such coatings are called columnar coatings and because the columns are connected only to the substrate and not to each other, the metallic substrate can ' expand and contract within reasonable limits without causing coating or spallation. Typical of this type of coating is that described in U.S. Patent 4,405,659.
  • the typical thickness of the ceramic thermal barrier coating would range from 10 mils to 50 mils (250 microns to 1250 microns), thicker coatings produce increased thermal barrier effects.
  • Blade root platforms are located on the blade rodt which is the thickest portion of the blade because the blade root is near the axis of rotation the centrifugal forces are more easily accommodated in the root than they are at the blade tip of the blade. Consequently, in this limited application thermal barrier coatings have been used with some success.
  • the invention is substantially different from the prior art thermal barrier coatings.
  • the invention in its basic form comprises many thin layers of ceramic applied to the superalloy substrate by an evaporation process. Usually there will be alternating layers of different ceramics applied to the substrate. The layers are separated by distinct interfaces or boundaries. These interfaces are a key feature of the invention.
  • an extremplary coating according to the present invention consists of alternating layers of yttria stabilized zirconia (in nanocrystalling form), and alumina with each layer being only about 1,000 angstroms thick.
  • a coating having a total thickness of between 4 microns to 5 microns results.
  • this coating exhibits only about half of the heat conduction which would be expected (by the rule of mixtures) based on the thermal conductivity properties of thick layers of yttria stabilized zirconia and alumina.
  • crystal structures of the same type which have substantially different lattice perimeters (a greater than 10% difference in lattice parameters), or
  • the layers be amorphous because we believe that amorphous layers contribute greatly to reduced heat conduction.
  • each layer may range in thickness from about 10 angstroms (1 nm) to about 10,000 angstroms (1,000 nm); and preferably each layer will range in thickness from about 50 angstroms (10 nm) to about 5,000 angstroms (500 nm).
  • a coating thickness of at least 1 mil (25 microns) is required and preferably at least 3 mils (75 microns) is required.
  • a maximum coating thickness is required for rotating components where coating weight is a critical factor and most prefer about 5 mils (125 microns) maximum thickness.
  • a coating thickness is required for stationary components, where weight is of less concern, there is no practical upper limit but generally coatings will not exceed about 12 mils (300 microns) in thickness.
  • Ceramic materials which appear to be ideally suited for use in coatings according to the present invention. These ceramic materials are alumina (AI2O3), stabilized zirconia, [preferably yttria stabilized zirconia (Zr0 2 plus Y2O3)], and ceria (Ce0 2 ]. We have done most of our work with the first two materials, alumina and yttria stabilized zirconia.
  • alumina In terms of inherent bulk thermal conductivity, alumina has the highest conductivity and ceria has the lowest conductivity while zirconia has an intermediate conductivity. In terms of oxygen permeability, yttria stabilized zirconia has the highest oxygen permeability, ceria has an intermediate oxygen permeability, and alumina has a low oxygen permeability. In general, a low oxygen permeability is desired since the coating will then tend to protect the underlying metallic substrate from oxidation by atmospheric oxygen which diffuses through the coating. In terms of hardness, alumina has the highest hardness, zirconia has an intermediate hardness and ceria has the lowest hardness. A high value of hardness is generally preferred because of problems with particle erosion which can occur in certain gas turbine applications.
  • alumina can be processed to have an amorphous characteristic while yttria stabilized zirconia and ceria are both generally crystalline materials. Consequently, it is desirable to have a significant number of the layers be alumina.
  • Alumina is preferred as the initial layer adjacent to the substrate; because the native oxide which forms on the substrate due to oxidation of the substrate will be alumina and it is felt that having an alumina layer in the coating adjacent to a naturally occurring alumina layer will probably provide the best coating adherence.
  • alumina In terms of crystal structure, alumina has a characteristic hexagonal structure, meaning that if it were deposited under conditions which encouraged the formation of a crystalline structure, that structure would be hexagonal. Under most deposition conditions alumina has a tendency to be amorphous.
  • the stabilized zirconia is a mixture of cubic and tetragonal lattices wherein the yttria tends to stabilize the cubic structure and sufficient yttria contents (more than about 20% by weight) will produce a fully stable structure.
  • Ceria has a cubic lattice structure.
  • the alumina materi- ⁇ tends to form an amorphous structure when it is vapor deposited onto a substrate which is held at a relatively low temperature ( ⁇ 2,000°F) and in the alternative it tends to form a crystalline structure when applied by a vapor deposition to a substrate held at a relatively high temperature (> 2,000°F).
  • the yttria stabilized zirconia may be either partially or fully stabilized. We have used partially stabilized yttria stabilized zirconia containing between 6 to 8 weight percent yttria because this is the material we currently use in plasma sprayed ceramic thermal barrier coatings and we have experience with its use and properties.
  • yttria may be used to stabilize the zirconia in which case the zirconia will be wholly stabilized and will not undergo any crystalline transformations with temperature changes.
  • Other materials such as cerium oxide, magnesium oxide, calcium oxide, and scandium oxide may also be used to stabilize zirconia.
  • the effective vapor pressure of one of the ceramic species drops dramatically as soon as the beam is switched away from one area to the other area and this means that there is very little grading of the inter layers in the resultant coatings.
  • alternating layers of ceramic were deposited by applying electrical current to independent sputter targets within the coating chamber.
  • One target was yttria stabilized zirconia and the second target was alumina.
  • the thickness of the deposited layer is proportional to the duration and density of applied current. The maintenance of sharp boundaries, even after long exposures at elevated temperatures, is encouraged with either process by the use of materials having low mutual solid solubilities.
  • the invention coating has been found to have other beneficial attributes. For example, in gas turbine engine components, fatigue damage from vibration is often a problem. The fatigue damage is effected by the vibrational modes exhibited by the article and these vibrational modes can be affected by surface coatings. We have found that the invention coating has no observable effect on the vibrational modes of the gas turbine engine components which we have investigated and this is desirable since it simplifies the calculation and analysis of vibrational modes and reduces the problems which would otherwise be encountered if the vibrational modes were to change as a function of coating thickness. Fatigue is also affected by residual surface stresses and we have not observed any detrimental residual stresses in the practice of the present invention.
  • the invention coating will commonly be applied to air cooled gas turbine superalloy components which have internal cooling passages connected to the component surface by many small cooling holes to allow air to flow from the internal passages to the surface of the part. Air flow over the surface of the part provides a protective air cooling film which prevents the hot engine gases from directly contacting the component surface. Whereas other thermal barrier coating techniques and other thermal barrier coating types tend to plug up these cooling passages and interfere with the air cooling flow, the present invention coatings have not been found to have any significant effect on airflow. This is a significant economic benefit.
  • thermal barrier coating of the present invention appears to fulfill the fundamental characteristics required of an effective thermal barrier coating for rotating gas turbine engine hardware, which are:
  • Superalloy test parts having a nominal composition (by weight) 5% Cr, 10% Co, 1.9% Mo, 5.9% w, 3.0% Re, 8.7% Ta, 5.65% Al, 0.10% Ht bal essentially Ni were cleaned and then coated with a layered coating comprising alternate layers of yttria stabilized zirconia (6.8% yttria) and alumina. Each layer was approximately 1,000 angstroms thick. The layered structure was examined by transmission electron microscopy and scanning electron microscopy and the interfaces were found to be sharp and distinct.
  • the coated parts were then tested for thermal conductivity using the 3-omega method developed by Cahill and described in D. G. Cahill et al Phys. Rev. B. vol. 35 pg. 4067 1987.
  • This method consists of depositing a thin metal line (platinum or gold, 3000 angstroms thick and 25 microns wide) on the surface of a coated sample using photolithography. Frequency dependent self-heating of the metal line, which acts as both heater and thermometer, is used to measure the thermal conductivity.
  • a thin metal line platinum or gold, 3000 angstroms thick and 25 microns wide
  • Frequency dependent self-heating of the metal line which acts as both heater and thermometer, is used to measure the thermal conductivity.
  • One advantage of this technique is that the thermal conductivity of the coating can be measured with no prior knowledge of other coating thermal properties (e.g., heat capacity).
  • the measured thermal conductivity of the laminated coating produced according to the present invention is only about one-half of the thermal conductivity calculated for a simple mixture of yttria stabilized zirconia and alumina using the rule of mixtures.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Physical Vapour Deposition (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)

Abstract

Un revêtement constituant une barrière thermique destiné à des applications à haute température présente une résistance accrue au flux thermique. Le revêtement se compose d'un grand nombre de ces couches (échelle nanométrique) séparées par des interfaces efficaces pour retarder le flux thermique. Le matériau de revêtement est typiquement une céramique à base d'oxyde et le revêtement trouve des applications particulières dans des turbines à gaz.
PCT/US1995/012771 1994-10-05 1995-10-04 Systeme de revetement par couches nanometriques multiples WO1996011288A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US32105294A 1994-10-05 1994-10-05
US321,052 1994-10-05

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WO1996011288A1 true WO1996011288A1 (fr) 1996-04-18

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Cited By (10)

* Cited by examiner, † Cited by third party
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EP1069205A1 (fr) * 1999-07-13 2001-01-17 General Electric Company Objet ayant un revêtement haute température modulable
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EP1072692A3 (fr) * 1999-07-28 2001-05-16 General Electric Company Méthode et assemblage pour évaluer la qualité d'un procédé de revêtement
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